CN116768220B - Method for rapidly synthesizing high-concentration non-spherical silica sol - Google Patents
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 31
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 14
- AVQQQNCBBIEMEU-UHFFFAOYSA-N 1,1,3,3-tetramethylurea Chemical compound CN(C)C(=O)N(C)C AVQQQNCBBIEMEU-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 29
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 24
- 229910052710 silicon Inorganic materials 0.000 claims description 24
- 239000010703 silicon Substances 0.000 claims description 24
- 239000003513 alkali Substances 0.000 claims description 22
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 20
- 239000012498 ultrapure water Substances 0.000 claims description 20
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical group [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 14
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 239000002585 base Substances 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 6
- 150000007530 organic bases Chemical class 0.000 claims description 5
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 4
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims description 4
- 150000007529 inorganic bases Chemical class 0.000 claims description 3
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 3
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 3
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 3
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 3
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims description 2
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 claims description 2
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 claims description 2
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 claims description 2
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims 4
- 238000003786 synthesis reaction Methods 0.000 claims 4
- 239000002245 particle Substances 0.000 abstract description 19
- 238000006243 chemical reaction Methods 0.000 abstract description 15
- 238000002360 preparation method Methods 0.000 abstract description 12
- 238000009826 distribution Methods 0.000 abstract description 11
- 229910021645 metal ion Inorganic materials 0.000 abstract description 7
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Chemical class 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 230000002572 peristaltic effect Effects 0.000 abstract description 3
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 2
- 150000004706 metal oxides Chemical class 0.000 abstract description 2
- 238000005580 one pot reaction Methods 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- 230000008961 swelling Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 17
- 230000005540 biological transmission Effects 0.000 description 14
- 238000001000 micrograph Methods 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 239000010410 layer Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 125000003916 ethylene diamine group Chemical group 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- -1 casting Substances 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses a method for rapidly synthesizing high-concentration non-spherical silica sol, and belongs to the technical field of silica sol materials. The invention selects tetramethyl urea as a deformation promoter, which plays roles of accelerating reaction and swelling silica sol particles in the process of generating silica sol, thereby realizing the one-pot synthesis of the special-shaped silica sol without controlling the feeding rate by additional instruments such as peristaltic pumps and the like. Meanwhile, metal oxides, metal salts and the like can be not used as catalysts, so that the pollution of metal ions to a system is avoided. The obtained silica sol has the advantages of high irregularity degree, narrow particle size distribution, good product stability, high concentration, no need of subsequent concentration to improve the concentration, simplified process flow, simple operation, greatly reduced preparation cost of the special-shaped silica sol, and suitability for large-scale practical application and popularization.
Description
Technical Field
The invention belongs to the technical field of silica sol materials, and particularly relates to a method for rapidly synthesizing high-concentration non-spherical silica sol.
Background
Silica sol is a colloidal substance obtained by dispersing silica particles in water or other solvents, and is widely used in the industries of papermaking, catalysts, casting, paints, and the like. With the high integration and high functionality of semiconductor integrated circuits, in order to prevent the problem that the roughness (height difference) of the layer surface exceeds the depth of focus of photolithography and a sufficient resolution cannot be obtained in the manufacture of semiconductor integrated circuits, an interlayer insulating film, buried wiring, and the like are planarized by a chemical mechanical polishing method.
Most of the current silica sol products are regular spherical products, and the research on non-spherical silica sol is relatively few. The spherical particles act like a bearing in the polishing process, the stress is easy to be conducted to the periphery, the roughness of the polishing surface can be effectively reduced, the damage is reduced, and the spherical particles are the most ideal abrasive material shape. However, the disadvantage is that the polishing rate is low, and it is difficult to meet the requirement of new material polishing.
The current preparation method of the non-spherical silica sol comprises the following steps: CN 115611286A, it discloses a preparation method of peanut-shaped ultra-high purity silica sol, ultra-high purity silica sol and application thereof, the main scheme is:
1) And (3) preparing a solution A: uniformly mixing an organic solvent, ultrapure water and a base catalyst in a certain proportion to ensure that the relative dielectric constant of the solution A is between 43 and 50;
2) And (3) preparing a solution B: uniformly mixing an organic solvent and alkoxy silane;
3) Initial silica sol preparation: adding the solution B into the solution A at a certain temperature, and stirring and reacting to obtain initial silica sol;
4) Concentrating: concentrating the initial silica sol to obtain a concentrated silica sol with the mass fraction of 10-20%; preferably, the concentration adopts a vacuum heating concentration mode;
5) Solvent replacement: replacing the organic solvent in the concentrated silica sol with ultrapure water, and concentrating to more than 20% by mass;
6) And (3) filtering: and filtering the concentrated silica sol to remove large particles, thereby obtaining the peanut-shaped ultra-high purity silica sol.
CN101402829a discloses potato-shaped silica sol and a preparation method thereof, which relates to potato-shaped silica sol and a preparation method thereof, comprising a liquid medium and silica colloid particles, and is characterized in that: the silica colloid particles are potato-shaped. The preparation method comprises the following steps: 1. preparing a starting sol: in the presence of SiO 2 Adding water-soluble calcium salt and magnesium salt aqueous solution into 1-6% active silicon aqueous solution in parts by weight; adding an alkali metal hydroxide water-soluble solution, heating and stirring the mixture to prepare an alkaline initial receiver sol, and preparing a potato-shaped sol solution: adding an active silicic acid solution into the initial sol; the preparation method adopts a liquid level particle growth method such as normal pressure.
However, there are various problems in the current prior art, such as:
1. in the preparation process, caO and MgO are used to introduce metal cations, the purity of the obtained silica sol is low, the metal cations are easy to cause the silica sol to gather and precipitate, the high-concentration silica sol cannot be synthesized, the morphology of the cut silica sol is unclear, and the shape of the cut silica sol is more similar to a sphere;
2. two solutions are required to be prepared, the feeding is carried out at a constant speed through a peristaltic pump, the steps are complicated, and an instrument for assisting the feeding is required.
Disclosure of Invention
Aiming at the problems in the prior art, the invention discloses a method for preparing high-concentration special-shaped silica sol by a one-step method, wherein the obtained silica sol has high purity, narrow particle size distribution, good product stability, simple preparation method, easy operation and greatly reduced production cost of special-shaped silica sol products.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a method for rapidly synthesizing high-concentration non-spherical silica sol comprises the following operation steps: adding tetramethylurea, alkali, a silicon source and ultrapure water into a container at one time, stirring and heating to obtain the non-spherical silica sol.
Further, the alkali is one or more of inorganic alkali and organic alkali.
Further, the inorganic base is ammonia water.
Still further, the organic base has a pka > 9.
Further, the organic base is one or more of ethylenediamine, propylenediamine, dimethylamine, trimethylamine, isopropylamine, tetraethylammonium hydroxide, tetramethylammonium hydroxide and tetrabutylammonium hydroxide.
Further, the silicon source is a siloxane.
Further, the siloxane is one or more of tetraethoxysilane, methyltrimethoxysilane, methyltriethoxysilane, phenyltrimethoxysilane, n-propyltrimethoxysilane, n-propyltriethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, vinyltrimethoxysilane and vinyltriethoxysilane.
Further, the mass ratio of tetramethylurea, alkali, silicon source and ultrapure water is (0.83-1.02): (0.0026 to 0.0053): (0.62 to 1.24): 1.
further, the temperature of stirring and heating is 60-150 ℃, the stirring rotation speed is 500rpm, and the heating time is 3-5h.
Advantageous effects
The invention selects tetramethyl urea as a deformation promoter, which plays roles of accelerating reaction and swelling silica sol particles in the process of generating silica sol, thereby realizing the one-pot synthesis of the special-shaped silica sol without controlling the feeding rate by additional instruments such as peristaltic pumps and the like. Meanwhile, metal oxides, metal salts and the like can be not used as catalysts, so that the pollution of metal ions to a system is avoided. The obtained silica sol has the advantages of high irregularity degree, narrow particle size distribution, good product stability, high concentration, no need of subsequent concentration to improve the concentration, simplified process flow, simple operation, greatly reduced preparation cost of the special-shaped silica sol, and suitability for large-scale practical application and popularization.
Drawings
FIG. 1 is a scanning electron microscope image of a silica sol obtained in example 1 of the present invention;
FIG. 2 is a transmission electron microscope image of the silica sol obtained in example 1 of the present invention;
FIG. 3 is a graph showing the particle size distribution of silica sol obtained in example 1 of the present invention;
FIG. 4 is a transmission electron microscope image of the silica sol obtained in example 2 of the present invention;
FIG. 5 is a graph showing the particle size distribution of silica sol obtained in example 2 of the present invention;
FIG. 6 is a transmission electron microscope image of the silica sol obtained in example 3 of the present invention;
FIG. 7 is a graph showing the particle size distribution of silica sol obtained in example 3 of the present invention;
FIG. 8 is a transmission electron microscope image of the silica sol obtained in example 4 of the present invention;
FIG. 9 is a particle size distribution chart of a silica sol obtained in example 4 of the present invention
FIG. 10 is a transmission electron microscopic view of the silica sol obtained in comparative example 1 of the present invention;
FIG. 11 is a graph showing the particle size distribution of the silica sol obtained in comparative example 1;
FIG. 12 is a transmission electron microscope image of the silica sol obtained in comparative example 2;
FIG. 13 is a graph showing the particle size distribution of the silica sol obtained in comparative example 2;
FIG. 14 is a transmission electron microscope image of the silica sol obtained in comparative example 3;
FIG. 15 is a graph showing the particle size distribution of the silica sol obtained in comparative example 3.
Detailed Description
The technical scheme of the present invention is further described below with reference to specific examples, but is not limited thereto.
Example 1
A method for rapidly synthesizing high-concentration non-spherical silica sol comprises the following operation steps: adding tetramethylurea, alkali, a silicon source and ultrapure water into a container at one time, stirring and heating to obtain the non-spherical silica sol.
The siloxane is tetraethoxysilane.
The base is ethylenediamine with a pka > 9.
The mass ratio of the tetramethylurea to the alkali to the silicon source to the ultrapure water is 1.017:0.004:1.058:1.
the temperature of stirring and heating is 80 ℃, the stirring rotation speed is 500rpm, and the heating time is 3-5h. And stopping heating after the tetraethoxysilane layer above the reaction system disappears, so as to obtain the non-spherical silica sol with the content of 9.4%. The scanning electron microscope image of the particles is shown in fig. 1, the transmission electron microscope image is shown in fig. 2, and the silica sol obtained by the method of the embodiment has higher irregularity, clear shape and uniform particle size, and can be seen from the particle size distribution diagram 3 as well.
Example 2
A method for rapidly synthesizing high-concentration non-spherical silica sol comprises the following operation steps: adding tetramethylurea, alkali, a silicon source and ultrapure water into a container at one time, stirring and heating to obtain the non-spherical silica sol.
The alkali is ammonia water.
The silicon source is siloxane, and specifically is methyltrimethoxysilane.
The mass ratio of tetramethylurea, alkali, silicon source and ultrapure water is 0.83:0.0026:0.62:1.
the temperature of stirring and heating is 60 ℃, the stirring rotation speed is 500rpm, and the heating time is 3-5h. And after the siloxane layer above the reaction system disappears, stopping heating after the reaction is finished, and obtaining the non-spherical silica sol with the content of 9.0 percent, wherein a transmission electron microscope chart is shown in figure 4.
Example 3
A method for rapidly synthesizing high-concentration non-spherical silica sol comprises the following operation steps: adding tetramethylurea, alkali, a silicon source and ultrapure water into a container at one time, stirring and heating to obtain the non-spherical silica sol.
The base is tetraethylammonium hydroxide.
The silicon source is siloxane, and specifically is methyltriethoxysilane.
The mass ratio of the tetramethylurea to the alkali to the silicon source to the ultrapure water is 1.02:0.0026:1.24:1.
the temperature of stirring and heating is 120 ℃, the stirring rotation speed is 500rpm, and the heating time is 3-5h. And after the siloxane layer above the reaction system disappears, stopping heating after the reaction is finished, and obtaining the non-spherical silica sol with the content of 10.2 percent, wherein a transmission electron microscope image is shown in figure 5.
Example 4
A method for rapidly synthesizing high-concentration non-spherical silica sol comprises the following operation steps: adding tetramethylurea, alkali, a silicon source and ultrapure water into a container at one time, stirring and heating to obtain the non-spherical silica sol.
The base is tetrabutylammonium hydroxide.
The silicon source is siloxane, and specifically phenyl trimethoxy silane.
The mass ratio of the tetramethylurea to the alkali to the silicon source to the ultrapure water is 1.02:0.0053:1.24:1.
the temperature of stirring and heating is 150 ℃, the stirring rotation speed is 500rpm, and the heating time is 3-5h. And after the siloxane layer above the reaction system disappears, stopping heating after the reaction is finished, and obtaining the non-spherical silica sol with the content of 10.0 percent, wherein a transmission electron microscope image is shown in figure 6.
Comparative example 1
A method for rapidly synthesizing high-concentration non-spherical silica sol comprises the following operation steps: adding ethanol, alkali, a silicon source and ultrapure water into a container at one time, stirring and heating to obtain the non-spherical silica sol.
The siloxane is tetraethoxysilane.
The base is ethylenediamine with a pka > 9.
The mass ratio of the ethanol to the alkali to the silicon source to the ultrapure water is 1.017:0.004:1.058:1.
the temperature of stirring and heating is 80 ℃, the stirring rotation speed is 500rpm, and the heating time is 3-5h. Stopping heating after the tetraethoxysilane layer above the reaction system disappears and the reaction is finished,
in this comparative example, the raw materials and the operation method were the same as in example 1, except that tetramethylurea was replaced with ethanol, a commonly used deforming agent. It can be seen from the transmission electron microscope image (fig. 10) that the morphology is substantially close to a sphere.
Comparative example 2
A method for rapidly synthesizing high-concentration non-spherical silica sol comprises the following operation steps: ammonia water, alkali, a silicon source and ultrapure water are added into a container at one time, and the non-spherical silica sol is obtained after stirring and heating.
The siloxane is tetraethoxysilane.
The base is ethylenediamine with a pka > 9.
The mass ratio of the ammonia water, the alkali, the silicon source and the ultrapure water is 1.017:0.004:1.058:1.
the temperature of stirring and heating is 80 ℃, the stirring rotation speed is 500rpm, and the heating time is 3-5h. Stopping heating after the tetraethoxysilane layer above the reaction system disappears and the reaction is finished,
in this comparative example, the raw materials and the operation method were the same as in example 1, except that tetramethylurea was replaced with aqueous ammonia as a conventional deforming agent. As can be seen from the transmission electron microscope image (fig. 12), the morphology is also substantially spherical.
Comparative example 3
A method for rapidly synthesizing high-concentration non-spherical silica sol comprises the following operation steps: adding a deforming agent, alkali, a silicon source and ultrapure water into a container at one time, stirring and heating to obtain the non-spherical silica sol.
The siloxane is tetraethoxysilane.
The base is ethylenediamine with a pka > 9.
The deforming agent is ammonia water and ethanol which are mixed in any proportion, and the comparative example is mixed in a ratio of 1:1.
The mass ratio of the deforming agent, the alkali, the silicon source and the ultrapure water is 1.017:0.004:1.058:1.
the temperature of stirring and heating is 80 ℃, the stirring rotation speed is 500rpm, and the heating time is 3-5h. Stopping heating after the tetraethoxysilane layer above the reaction system disappears and the reaction is finished,
in this comparative example, the raw materials and the operation method were the same as in example 1, except that tetramethylurea was replaced with ammonia and ethanol, which are commonly used as the deforming agents. As can be seen from the transmission electron microscope image (fig. 14), the morphology is also substantially spherical.
Metal ion content test, ICP-MS measures the metal cation content of the product, and the test results are shown in table 1:
TABLE 1 results of Metal ion Performance test
| Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Fe(ppb) | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected |
| Zn(ppb) | 300 | 200 | 200 | 300 | 300 | 300 | 300 |
| Na (ppb) | 2000 | 1000 | 1000 | 2000 | 2000 | 1500 | 2000 |
| K(ppb) | 4000 | 5000 | 4000 | 4000 | 4000 | 4000 | 4000 |
| Ca(ppb) | 300 | 100 | 200 | 200 | 300 | 300 | 300 |
| Mg(ppb) | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected |
| Al(ppb) | 500 | 500 | 500 | 400 | 500 | 500 | 500 |
| Cu(ppb) | 700 | 600 | 700 | 700 | 700 | 800 | 800 |
| Pb（wt%） | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected |
| Co(wt%) | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected |
| Mn (wt%) | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected |
| Ti (wt%) | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected |
| Ni (wt%) | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected |
| Cr (wt%) | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected |
| Ag (wt%) | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected | Not detected |
As can be seen from the metal ion detection test data of the invention, the silica sol products obtained by the embodiment and the comparative example have little change of the metal ion content, and can meet the actual use requirements. The preparation process of the invention basically avoids the introduction of metal ions, and the method is simple and efficient.
It should be noted that the above-mentioned embodiments are merely some, but not all embodiments of the preferred mode of carrying out the invention. It is evident that all other embodiments obtained by a person skilled in the art without making any inventive effort, based on the above-described embodiments of the invention, shall fall within the scope of protection of the invention.
Claims (6)
1. A method for rapidly synthesizing high-concentration non-spherical silica sol is characterized by comprising the following operation steps: adding tetramethylurea, alkali, a silicon source and ultrapure water into a container at one time, stirring and heating to obtain non-spherical silica sol;
the silicon source is siloxane; the mass ratio of the tetramethylurea to the alkali to the silicon source to the ultrapure water is (0.83-1.02): (0.0026 to 0.0053): (0.62 to 1.24): 1, a step of; the temperature of stirring and heating is 60-150 ℃, the stirring rotation speed is 500rpm, and the heating time is 3-5h.
2. The method for rapid synthesis of high concentration non-spherical silica sol according to claim 1, wherein the base is one or more of inorganic base or organic base.
3. The method for rapid synthesis of high concentration non-spherical silica sol according to claim 2, wherein the inorganic base is ammonia water.
4. The method for rapid synthesis of high concentration non-spherical silica sol according to claim 2, wherein the organic base has a pka > 9.
5. The method for rapid synthesis of high concentration non-spherical silica sol according to claim 4, wherein the organic base is one or more of ethylenediamine, propylenediamine, dimethylamine, trimethylamine, isopropylamine, tetraethylammonium hydroxide, tetramethylammonium hydroxide, tetrabutylammonium hydroxide.
6. The method for rapidly synthesizing high-concentration non-spherical silica sol according to claim 1, wherein the siloxane is one or more of tetraethoxysilane, methyltrimethoxysilane, methyltriethoxysilane, phenyltrimethoxysilane, n-propyltrimethoxysilane, n-propyltriethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, vinyltrimethoxysilane, and vinyltriethoxysilane.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310806510.7A CN116768220B (en) | 2023-07-04 | 2023-07-04 | Method for rapidly synthesizing high-concentration non-spherical silica sol |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310806510.7A CN116768220B (en) | 2023-07-04 | 2023-07-04 | Method for rapidly synthesizing high-concentration non-spherical silica sol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116768220A CN116768220A (en) | 2023-09-19 |
| CN116768220B true CN116768220B (en) | 2023-12-29 |
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| JP2009161371A (en) * | 2007-12-28 | 2009-07-23 | Jgc Catalysts & Chemicals Ltd | Silica sol and manufacturing method thereof |
| JP2009188059A (en) * | 2008-02-04 | 2009-08-20 | Nippon Chem Ind Co Ltd | Polishing colloidal silica for semiconductor wafer, and method for producing same |
| CN103408027A (en) * | 2013-07-11 | 2013-11-27 | 江苏天恒纳米科技有限公司 | Preparation method and application of silica sol with irregular shape |
| CN107473234A (en) * | 2017-09-27 | 2017-12-15 | 山东银丰纳米新材料有限公司 | A kind of preparation method of Ludox for CMP |
| CN116143126A (en) * | 2022-12-29 | 2023-05-23 | 临沂市科翰硅制品有限公司 | Process for preparing anisotropically grown shaped silica particles |
| CN116216728A (en) * | 2023-01-03 | 2023-06-06 | 万华化学集团股份有限公司 | Compact special-shaped colloidal silicon dioxide and preparation method and application thereof |
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| TW575656B (en) * | 2001-12-07 | 2004-02-11 | Chung Shan Inst Of Science | A method for preparing shape-changed nanosize colloidal silica |
| JP5602358B2 (en) * | 2007-11-30 | 2014-10-08 | 日揮触媒化成株式会社 | Non-spherical silica sol, method for producing the same, and polishing composition |
| CN111788154B (en) * | 2018-02-26 | 2024-03-29 | 日产化学株式会社 | Method for producing silica sol having elongated particle shape |
| JP7254603B2 (en) * | 2019-04-22 | 2023-04-10 | 扶桑化学工業株式会社 | Colloidal silica for metal polishing |
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|---|---|---|---|---|
| JP2009161371A (en) * | 2007-12-28 | 2009-07-23 | Jgc Catalysts & Chemicals Ltd | Silica sol and manufacturing method thereof |
| JP2009188059A (en) * | 2008-02-04 | 2009-08-20 | Nippon Chem Ind Co Ltd | Polishing colloidal silica for semiconductor wafer, and method for producing same |
| CN103408027A (en) * | 2013-07-11 | 2013-11-27 | 江苏天恒纳米科技有限公司 | Preparation method and application of silica sol with irregular shape |
| CN107473234A (en) * | 2017-09-27 | 2017-12-15 | 山东银丰纳米新材料有限公司 | A kind of preparation method of Ludox for CMP |
| CN116143126A (en) * | 2022-12-29 | 2023-05-23 | 临沂市科翰硅制品有限公司 | Process for preparing anisotropically grown shaped silica particles |
| CN116216728A (en) * | 2023-01-03 | 2023-06-06 | 万华化学集团股份有限公司 | Compact special-shaped colloidal silicon dioxide and preparation method and application thereof |
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| CN116768220A (en) | 2023-09-19 |
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